+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0259 started at 17:33:10 on 16-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0259 in P2(1) CELL 0.71073 9.7832 10.0420 11.5984 90.000 109.228 90.000 ZERR 2.00 0.0002 0.0002 0.0002 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O P CL UNIT 36 50 10 4 6 2 V = 1075.90 F(000) = 492.0 Mu = 0.43 mm-1 Cell Wt = 943.58 Rho = 1.456 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 OMIT -1 2 1 OMIT 2 1 0 OMIT -1 -2 1 OMIT 0 0 2 OMIT 2 0 1 OMIT -1 -1 1 ISOR 0.001 C5' FMAP 2 PLAN 20 SIZE 0.20 0.20 0.30 ACTA BOND WGHT 0.07520 0.53740 L.S. 5 TEMP -153.00 FVAR 1.17662 0.73088 C1 1 0.268725 0.412276 0.924553 11.00000 0.01905 0.01848 = 0.02431 0.00139 0.01726 0.00037 AFIX 23 H1A 2 0.238031 0.351455 0.978597 11.00000 -1.20000 H1B 2 0.191703 0.412000 0.843804 11.00000 -1.20000 AFIX 0 C2 1 0.281999 0.553026 0.977435 11.00000 0.02562 0.01944 = 0.02208 -0.00212 0.01805 -0.00090 AFIX 23 H2A 2 0.197973 0.568832 1.005279 11.00000 -1.20000 H2B 2 0.369982 0.556284 1.050533 11.00000 -1.20000 AFIX 0 C3 1 0.289880 0.667546 0.893575 11.00000 0.01648 0.01383 = 0.02574 -0.00286 0.01264 0.00167 AFIX 23 H3A 2 0.216773 0.653703 0.812014 11.00000 -1.20000 H3B 2 0.266838 0.752119 0.927014 11.00000 -1.20000 AFIX 0 C4 1 0.433864 0.874321 0.660152 11.00000 0.03148 0.02279 = 0.06688 0.02664 -0.01554 -0.01053 AFIX 23 H4A 2 0.478837 0.902485 0.746185 11.00000 -1.20000 H4B 2 0.351423 0.934441 0.620966 11.00000 -1.20000 AFIX 0 PART 1 C5 1 0.556837 0.884397 0.586352 21.00000 0.00998 0.05552 = 0.05059 -0.04823 -0.00274 0.00270 AFIX 23 H5A 2 0.640163 0.825727 0.626853 21.00000 -1.20000 H5B 2 0.512397 0.853749 0.501008 21.00000 -1.20000 AFIX 0 PART 2 C5' 1 0.559723 0.939288 0.678450 -21.00000 0.00323 0.00293 = 0.00355 0.00025 0.00084 -0.00076 AFIX 23 H5'1 2 0.635997 0.870969 0.709470 -21.00000 -1.20000 H5'2 2 0.569139 1.000058 0.747858 -21.00000 -1.20000 AFIX 0 PART 0 C6 1 0.606943 1.021424 0.587185 11.00000 0.06402 0.04640 = 0.05149 0.00374 0.02444 -0.00406 AFIX 23 H6A 2 0.529108 1.077745 0.532929 11.00000 -1.20000 H6B 2 0.635724 1.058555 0.670855 11.00000 -1.20000 AFIX 0 C7 1 0.803374 0.445720 0.709459 11.00000 0.00923 0.02360 = 0.01006 0.00161 0.00384 0.00095 C8 1 0.862524 0.558067 0.672157 11.00000 0.02762 0.03007 = 0.02427 -0.00022 0.01528 -0.00495 AFIX 43 H8 2 0.844903 0.644383 0.697705 11.00000 -1.20000 AFIX 0 C9 1 0.947166 0.542577 0.597535 11.00000 0.03213 0.05580 = 0.02778 0.00234 0.01950 -0.01285 AFIX 43 H9 2 0.986821 0.619027 0.572079 11.00000 -1.20000 AFIX 0 C10 1 0.974477 0.418786 0.559971 11.00000 0.01833 0.07020 = 0.01768 -0.00241 0.01135 0.00190 AFIX 43 H10 2 1.033638 0.409598 0.509881 11.00000 -1.20000 AFIX 0 C11 1 0.915245 0.307504 0.595569 11.00000 0.02560 0.04965 = 0.01682 -0.00457 0.00818 0.01497 AFIX 43 H11 2 0.933226 0.221833 0.568912 11.00000 -1.20000 AFIX 0 C12 1 0.829101 0.319562 0.670415 11.00000 0.02029 0.02499 = 0.01897 -0.00082 0.00965 0.00618 AFIX 43 H12 2 0.788593 0.242702 0.694372 11.00000 -1.20000 AFIX 0 C13 1 0.834541 0.457645 0.963899 11.00000 0.00941 0.01258 = 0.01455 0.00236 0.00616 -0.00115 C14 1 0.946466 0.364152 0.991498 11.00000 0.01156 0.02259 = 0.01513 0.00385 0.00675 0.00192 AFIX 43 H14 2 0.957743 0.308848 0.928787 11.00000 -1.20000 AFIX 0 C15 1 1.041286 0.351633 1.110062 11.00000 0.00905 0.03306 = 0.01970 0.00778 0.00367 0.00438 AFIX 43 H15 2 1.117110 0.287808 1.128244 11.00000 -1.20000 AFIX 0 C16 1 1.025442 0.432449 1.202353 11.00000 0.02045 0.04053 = 0.01406 -0.00104 0.00088 -0.00312 AFIX 43 H16 2 1.090735 0.424260 1.283375 11.00000 -1.20000 AFIX 0 C17 1 0.913790 0.525201 1.175642 11.00000 0.03230 0.03403 = 0.01723 -0.01050 0.00404 0.00199 AFIX 43 H17 2 0.902387 0.580074 1.238576 11.00000 -1.20000 AFIX 0 C18 1 0.818247 0.537755 1.056148 11.00000 0.02224 0.01883 = 0.02191 -0.00406 0.00556 0.00293 AFIX 43 H18 2 0.742060 0.601202 1.038051 11.00000 -1.20000 AFIX 0 N1 3 0.360972 0.494826 0.709374 11.00000 0.01142 0.00929 = 0.01036 0.00094 0.00282 0.00108 N2 3 0.626786 0.609599 0.793661 11.00000 0.01020 0.00844 = 0.01909 0.00045 0.00417 0.00007 N3 3 0.598204 0.335408 0.798269 11.00000 0.01144 0.00748 = 0.01924 0.00150 0.00636 0.00222 N4 3 0.403077 0.359865 0.909982 11.00000 0.01535 0.01824 = 0.01718 0.00702 0.00961 0.00569 N5 3 0.383041 0.739340 0.655765 11.00000 0.01632 0.01253 = 0.01678 0.00746 0.00267 0.00149 O1 4 0.433149 0.677222 0.881306 11.00000 0.01372 0.01354 = 0.01393 -0.00546 0.00690 -0.00233 O2 4 0.721540 1.017942 0.547001 11.00000 0.04676 0.07528 = 0.01171 0.00431 0.00715 0.02823 AFIX 147 H2 2 0.699115 0.976079 0.480668 11.00000 -1.50000 AFIX 0 P1 5 0.433414 0.362732 0.780372 11.00000 0.00907 0.00764 = 0.01270 -0.00084 0.00471 -0.00057 P2 5 0.455960 0.625974 0.758407 11.00000 0.00923 0.00750 = 0.00976 0.00092 0.00369 0.00109 P3 5 0.701650 0.464821 0.812873 11.00000 0.00802 0.00986 = 0.01236 0.00115 0.00471 0.00069 CL1 6 0.319593 0.212115 0.673952 11.00000 0.01797 0.01167 = 0.03298 -0.00839 0.00669 -0.00474 H5N 2 0.347972 0.708833 0.582293 11.00000 0.02829 H4N 2 0.450575 0.306933 0.959024 11.00000 0.02311 HKLF 4 Covalent radii and connectivity table for 2007src0259 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 CL 0.990 C1 - N4 C2 C2 - C3 C1 C3 - O1 C2 C4 - C5'_b N5 C5_a C5_a - C6 C4 C5'_b - C4 C6 C6 - O2 C5_a C5'_b C7 - C12 C8 P3 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C7 C11 C13 - C18 C14 P3 C14 - C15 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C13 C17 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C1 P1 N5 - C4 P2 O1 - C3 P2 O2 - C6 P1 - N3 N1 N4 Cl1 P2 P2 - N2 O1 N1 N5 P1 P3 - N2 N3 C7 C13 Cl1 - P1 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 5 0 4.70 1.08 observed but should be systematically absent 15417 Reflections read, of which 24 rejected -12 =< h =< 12, -13 =< k =< 12, -14 =< l =< 15, Max. 2-theta = 54.99 1 Systematic absence violations 0 Inconsistent equivalents 4883 Unique reflections, of which 0 suppressed R(int) = 0.0237 R(sigma) = 0.0270 Friedel opposites not merged Maximum memory for data reduction = 2713 / 48769 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3495 / 352404 wR2 = 0.1021 before cycle 1 for 4883 data and 281 / 281 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.027 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18891 0.00211 5.813 OSF 2 0.72012 0.00838 -1.285 FVAR 2 Mean shift/esd = 0.365 Maximum = 5.813 for OSF Max. shift = 0.037 A for H5N Max. dU = 0.002 for H5N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3495 / 352404 wR2 = 0.1013 before cycle 2 for 4883 data and 281 / 281 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 GooF = S = 1.019; Restrained GooF = 1.019 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19238 0.00211 1.646 OSF 2 0.71839 0.00834 -0.208 FVAR 2 Mean shift/esd = 0.131 Maximum = 1.646 for OSF Max. shift = 0.017 A for H5N Max. dU = 0.001 for H5N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3495 / 352404 wR2 = 0.1012 before cycle 3 for 4883 data and 281 / 281 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 GooF = S = 1.018; Restrained GooF = 1.017 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19251 0.00211 0.060 OSF 2 0.71860 0.00832 0.026 FVAR 2 Mean shift/esd = 0.020 Maximum = -0.458 for U23 C5_a Max. shift = 0.002 A for H4N Max. dU = 0.001 for C5_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 3495 / 352404 wR2 = 0.1012 before cycle 4 for 4883 data and 281 / 281 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 GooF = S = 1.018; Restrained GooF = 1.017 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19256 0.00211 0.023 OSF 2 0.71906 0.00833 0.054 FVAR 2 Mean shift/esd = 0.014 Maximum = -0.276 for U23 C5_a Max. shift = 0.002 A for C5_a Max. dU = 0.000 for C5_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 3495 / 352404 wR2 = 0.1012 before cycle 5 for 4883 data and 281 / 281 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 GooF = S = 1.018; Restrained GooF = 1.017 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19259 0.00211 0.013 OSF 2 0.71940 0.00832 0.042 FVAR 2 Mean shift/esd = 0.009 Maximum = -0.227 for U23 C5_a Max. shift = 0.001 A for C5_a Max. dU = 0.000 for C5_a Largest correlation matrix elements 0.767 U33 C5'_b / U22 C5'_b 0.609 U13 C5'_b / U11 C5'_b 0.556 U13 C2 / U33 C2 0.767 U22 C5'_b / U11 C5'_b -0.607 U23 C5_a / U22 C5_a 0.548 U13 C1 / U11 C1 0.767 U33 C5'_b / U11 C5'_b 0.606 U13 C5'_b / U33 C5'_b 0.543 U13 C1 / U33 C1 -0.700 U33 C5'_b / FVAR 2 0.574 U13 C5'_b / U22 C5'_b 0.520 U13 C9 / U33 C9 -0.695 U11 C5'_b / FVAR 2 0.561 U13 C2 / U11 C2 0.520 U13 C9 / U11 C9 -0.684 U22 C5'_b / FVAR 2 -0.559 U23 C5_a / U33 C5_a 0.509 U13 N4 / U33 N4 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.2380 0.3514 0.9785 23 0.990 0.000 C1 N4 C2 H1B 0.1917 0.4120 0.8437 23 0.990 0.000 C1 N4 C2 H2A 0.1980 0.5687 1.0052 23 0.990 0.000 C2 C3 C1 H2B 0.3700 0.5562 1.0505 23 0.990 0.000 C2 C3 C1 H3A 0.2168 0.6538 0.8119 23 0.990 0.000 C3 O1 C2 H3B 0.2668 0.7522 0.9269 23 0.990 0.000 C3 O1 C2 H4A 0.4794 0.9024 0.7464 23 0.990 0.000 C4 N5 C5_a H4B 0.3515 0.9347 0.6216 23 0.990 0.000 C4 N5 C5_a H5A 0.6402 0.8265 0.6255 23 0.990 0.001 C5_a C6 C4 H5B 0.5120 0.8556 0.5002 23 0.990 0.001 C5_a C6 C4 H5'1 0.6360 0.8713 0.7099 23 0.990 0.000 C5'_b C4 C6 H5'2 0.5689 1.0008 0.7473 23 0.990 0.000 C5'_b C4 C6 H6A 0.5291 1.0770 0.5333 23 0.990 0.000 C6 O2 C5_a H6B 0.6357 1.0570 0.6710 23 0.990 0.000 C6 O2 C5_a H8 0.8449 0.6441 0.6978 43 0.950 0.000 C8 C9 C7 H9 0.9866 0.6191 0.5721 43 0.950 0.000 C9 C10 C8 H10 1.0335 0.4097 0.5099 43 0.950 0.000 C10 C9 C11 H11 0.9334 0.2217 0.5691 43 0.950 0.000 C11 C10 C12 H12 0.7886 0.2430 0.6944 43 0.950 0.000 C12 C7 C11 H14 0.9578 0.3092 0.9288 43 0.950 0.000 C14 C15 C13 H15 1.1172 0.2882 1.1283 43 0.950 0.000 C15 C14 C16 H16 1.0909 0.4246 1.2834 43 0.950 0.000 C16 C17 C15 H17 0.9022 0.5796 1.2387 43 0.950 0.000 C17 C16 C18 H18 0.7420 0.6011 1.0381 43 0.950 0.000 C18 C13 C17 H2 0.6985 0.9769 0.4800 147 0.840 0.000 O2 C6 H2 2007src0259 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.26876 0.41223 0.92448 1.00000 0.01977 0.01919 0.02472 0.00157 0.01744 0.00039 0.01874 0.00528 0.00027 0.00025 0.00024 0.00000 0.00114 0.00114 0.00116 0.00095 0.00097 0.00091 0.00048 H1A 0.23803 0.35141 0.97850 1.00000 0.02248 0.00000 0.00000 H1B 0.19174 0.41199 0.84373 1.00000 0.02248 0.00000 0.00000 C2 0.28201 0.55293 0.97738 1.00000 0.02593 0.02032 0.02265 -0.00212 0.01819 -0.00091 0.02046 0.00527 0.00028 0.00025 0.00023 0.00000 0.00125 0.00123 0.00118 0.00098 0.00103 0.00098 0.00050 H2A 0.19799 0.56871 1.00524 1.00000 0.02455 0.00000 0.00000 H2B 0.37000 0.55618 1.05048 1.00000 0.02455 0.00000 0.00000 C3 0.28987 0.66759 0.89347 1.00000 0.01706 0.01445 0.02626 -0.00295 0.01275 0.00164 0.01787 0.00504 0.00026 0.00024 0.00023 0.00000 0.00107 0.00107 0.00120 0.00089 0.00093 0.00082 0.00046 H3A 0.21676 0.65377 0.81191 1.00000 0.02144 0.00000 0.00000 H3B 0.26684 0.75215 0.92693 1.00000 0.02144 0.00000 0.00000 C4 0.43405 0.87449 0.66034 1.00000 0.03247 0.02311 0.06768 0.02685 -0.01572 -0.01026 0.04902 0.00687 0.00036 0.00033 0.00038 0.00000 0.00155 0.00153 0.00236 0.00159 0.00156 0.00129 0.00105 H4A_a 0.47941 0.90238 0.74641 1.00000 0.05883 0.00000 0.00000 H4B_a 0.35149 0.93466 0.62164 1.00000 0.05883 0.00000 0.00000 C5_a 0.55695 0.88556 0.58573 0.71940 0.00901 0.05811 0.05287 -0.05189 -0.00328 0.00318 0.04331 0.00690 0.00038 0.00051 0.00044 0.00832 0.00161 0.00309 0.00272 0.00245 0.00157 0.00166 0.00156 H5A_a 0.64019 0.82652 0.62550 0.71940 0.05197 0.00832 0.00000 H5B_a 0.51200 0.85562 0.50022 0.71940 0.05197 0.00832 0.00000 C5'_b 0.55967 0.93943 0.67829 0.28060 0.00571 0.00529 0.00619 0.00041 0.00162 -0.00102 0.00581 0.01360 0.00072 0.00070 0.00061 0.00832 0.00201 0.00203 0.00202 0.00094 0.00106 0.00094 0.00185 H5'1_b 0.63603 0.87130 0.70986 0.28060 0.00697 0.00832 0.00000 H5'2_b 0.56885 1.00076 0.74727 0.28060 0.00697 0.00832 0.00000 C6 0.60683 1.02036 0.58716 1.00000 0.06461 0.04812 0.05225 0.00499 0.02483 -0.00237 0.05362 0.00906 0.00048 0.00044 0.00039 0.00000 0.00245 0.00235 0.00217 0.00180 0.00192 0.00194 0.00097 H6A_a 0.52909 1.07705 0.53326 1.00000 0.06434 0.00000 0.00000 H6B_a 0.63571 1.05697 0.67102 1.00000 0.06434 0.00000 0.00000 C7 0.80344 0.44575 0.70953 1.00000 0.00963 0.02445 0.01066 0.00156 0.00396 0.00102 0.01476 0.00457 0.00023 0.00026 0.00019 0.00000 0.00092 0.00119 0.00087 0.00087 0.00075 0.00084 0.00043 C8 0.86252 0.55778 0.67221 1.00000 0.02812 0.03087 0.02489 -0.00027 0.01547 -0.00459 0.02630 0.00579 0.00031 0.00031 0.00025 0.00000 0.00133 0.00144 0.00126 0.00108 0.00108 0.00113 0.00056 H8 0.84490 0.64407 0.69782 1.00000 0.03156 0.00000 0.00000 C9 0.94710 0.54260 0.59756 1.00000 0.03282 0.05699 0.02831 0.00229 0.01978 -0.01318 0.03698 0.00665 0.00034 0.00040 0.00028 0.00000 0.00151 0.00210 0.00141 0.00144 0.00125 0.00152 0.00073 H9 0.98665 0.61911 0.57210 1.00000 0.04438 0.00000 0.00000 C10 0.97441 0.41886 0.56002 1.00000 0.01891 0.07148 0.01811 -0.00266 0.01139 0.00182 0.03486 0.00632 0.00030 0.00039 0.00024 0.00000 0.00124 0.00242 0.00118 0.00134 0.00102 0.00134 0.00077 H10 1.03352 0.40972 0.50988 1.00000 0.04184 0.00000 0.00000 C11 0.91531 0.30744 0.59566 1.00000 0.02631 0.05030 0.01732 -0.00476 0.00830 0.01466 0.03103 0.00614 0.00030 0.00035 0.00024 0.00000 0.00131 0.00184 0.00116 0.00118 0.00104 0.00128 0.00066 H11 0.93335 0.22173 0.56912 1.00000 0.03724 0.00000 0.00000 C12 0.82919 0.31984 0.67044 1.00000 0.02077 0.02558 0.01953 -0.00064 0.00981 0.00590 0.02118 0.00528 0.00027 0.00028 0.00022 0.00000 0.00112 0.00128 0.00111 0.00096 0.00097 0.00095 0.00050 H12 0.78860 0.24302 0.69438 1.00000 0.02542 0.00000 0.00000 C13 0.83457 0.45763 0.96388 1.00000 0.00994 0.01298 0.01524 0.00241 0.00619 -0.00134 0.01222 0.00433 0.00022 0.00022 0.00019 0.00000 0.00088 0.00100 0.00094 0.00082 0.00075 0.00080 0.00040 C14 0.94642 0.36445 0.99152 1.00000 0.01223 0.02304 0.01586 0.00357 0.00703 0.00185 0.01645 0.00488 0.00024 0.00027 0.00021 0.00000 0.00091 0.00114 0.00099 0.00091 0.00081 0.00092 0.00043 H14 0.95779 0.30917 0.92882 1.00000 0.01974 0.00000 0.00000 C15 1.04134 0.35195 1.11018 1.00000 0.00974 0.03383 0.02073 0.00774 0.00412 0.00445 0.02165 0.00522 0.00024 0.00030 0.00022 0.00000 0.00096 0.00139 0.00113 0.00106 0.00086 0.00099 0.00050 H15 1.11720 0.28815 1.12834 1.00000 0.02598 0.00000 0.00000 C16 1.02551 0.43264 1.20238 1.00000 0.02122 0.04127 0.01463 -0.00107 0.00105 -0.00326 0.02690 0.00535 0.00029 0.00032 0.00023 0.00000 0.00121 0.00167 0.00103 0.00112 0.00092 0.00114 0.00058 H16 1.09093 0.42462 1.28338 1.00000 0.03228 0.00000 0.00000 C17 0.91376 0.52498 1.17568 1.00000 0.03301 0.03471 0.01805 -0.01067 0.00456 0.00167 0.02954 0.00550 0.00031 0.00032 0.00024 0.00000 0.00141 0.00159 0.00116 0.00109 0.00106 0.00120 0.00061 H17 0.90216 0.57964 1.23866 1.00000 0.03545 0.00000 0.00000 C18 0.81822 0.53767 1.05618 1.00000 0.02282 0.01930 0.02269 -0.00388 0.00583 0.00267 0.02201 0.00509 0.00027 0.00027 0.00023 0.00000 0.00121 0.00118 0.00117 0.00099 0.00097 0.00100 0.00050 H18 0.74203 0.60112 1.03812 1.00000 0.02642 0.00000 0.00000 N1 0.36099 0.49478 0.70932 1.00000 0.01197 0.00993 0.01082 0.00090 0.00291 0.00095 0.01112 0.00352 0.00019 0.00019 0.00016 0.00000 0.00080 0.00081 0.00077 0.00068 0.00066 0.00068 0.00035 N2 0.62679 0.60951 0.79362 1.00000 0.01106 0.00912 0.01973 0.00048 0.00446 -0.00015 0.01345 0.00385 0.00020 0.00019 0.00018 0.00000 0.00082 0.00084 0.00089 0.00072 0.00071 0.00070 0.00036 N3 0.59820 0.33554 0.79820 1.00000 0.01227 0.00804 0.01999 0.00157 0.00663 0.00225 0.01311 0.00386 0.00020 0.00018 0.00018 0.00000 0.00084 0.00084 0.00092 0.00069 0.00072 0.00066 0.00037 N4 0.40299 0.35976 0.90989 1.00000 0.01607 0.01873 0.01808 0.00719 0.00985 0.00576 0.01659 0.00435 0.00021 0.00023 0.00019 0.00000 0.00089 0.00097 0.00092 0.00085 0.00075 0.00082 0.00038 N5 0.38306 0.73938 0.65591 1.00000 0.01700 0.01324 0.01714 0.00725 0.00263 0.00125 0.01653 0.00435 0.00022 0.00020 0.00020 0.00000 0.00094 0.00100 0.00100 0.00076 0.00077 0.00073 0.00041 O1 0.43306 0.67723 0.88124 1.00000 0.01449 0.01434 0.01462 -0.00532 0.00714 -0.00212 0.01391 0.00308 0.00017 0.00016 0.00014 0.00000 0.00075 0.00081 0.00073 0.00061 0.00061 0.00059 0.00033 O2 0.72123 1.01748 0.54699 1.00000 0.04751 0.07659 0.01253 0.00444 0.00756 0.02880 0.04611 0.00536 0.00026 0.00031 0.00018 0.00000 0.00131 0.00197 0.00084 0.00103 0.00085 0.00136 0.00069 H2 0.69851 0.97686 0.48000 1.00000 0.06917 0.00000 0.00000 P1 0.43341 0.36272 0.78036 1.00000 0.00969 0.00822 0.01332 -0.00082 0.00491 -0.00058 0.01014 0.00104 0.00005 0.00005 0.00005 0.00000 0.00024 0.00025 0.00026 0.00019 0.00020 0.00019 0.00013 P2 0.45595 0.62596 0.75840 1.00000 0.00982 0.00813 0.01036 0.00094 0.00388 0.00112 0.00930 0.00104 0.00006 0.00005 0.00005 0.00000 0.00024 0.00025 0.00023 0.00020 0.00019 0.00019 0.00012 P3 0.70166 0.46483 0.81287 1.00000 0.00858 0.01042 0.01296 0.00115 0.00489 0.00068 0.01032 0.00105 0.00006 0.00005 0.00005 0.00000 0.00023 0.00027 0.00025 0.00019 0.00019 0.00019 0.00013 Cl1 0.31959 0.21212 0.67400 1.00000 0.01859 0.01224 0.03372 -0.00839 0.00694 -0.00472 0.02193 0.00112 0.00006 0.00006 0.00006 0.00000 0.00026 0.00025 0.00033 0.00023 0.00023 0.00021 0.00014 H5N 0.34853 0.70800 0.58726 1.00000 0.03155 0.07461 0.00380 0.00397 0.00343 0.00000 0.00918 H4N 0.44877 0.30448 0.95698 1.00000 0.02395 0.06480 0.00357 0.00362 0.00302 0.00000 0.00841 Final Structure Factor Calculation for 2007src0259 in P2(1) Total number of l.s. parameters = 281 Maximum vector length = 511 Memory required = 3216 / 27090 wR2 = 0.1012 before cycle 6 for 4883 data and 2 / 281 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 GooF = S = 1.018; Restrained GooF = 1.017 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0752 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0340 for 4795 Fo > 4sig(Fo) and 0.0348 for all 4883 data wR2 = 0.1012, GooF = S = 1.018, Restrained GooF = 1.017 for all data Flack x parameter = 0.5078 with esd 0.0629 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0303 0.0191 0.0068 C1 0.0324 0.0202 0.0088 C2 0.0279 0.0165 0.0092 C3 0.1149 0.0217 0.0104 C4 0.1170 0.0096 0.0034 C5_a 0.0072 0.0058 0.0044 C5'_b 0.0655 0.0542 0.0412 C6 0.0246 0.0106 0.0090 C7 0.0350 0.0284 0.0155 C8 0.0630 0.0359 0.0121 C9 0.0717 0.0225 0.0104 C10 0.0593 0.0215 0.0123 C11 0.0296 0.0211 0.0129 C12 0.0168 0.0129 0.0070 C13 0.0247 0.0149 0.0098 C14 0.0374 0.0186 0.0089 C15 0.0418 0.0258 0.0131 C16 0.0438 0.0320 0.0128 C17 0.0287 0.0216 0.0158 C18 0.0129 0.0114 0.0091 N1 0.0203 0.0110 0.0091 N2 0.0202 0.0121 0.0071 N3 0.0276 0.0116 0.0106 N4 0.0247 0.0173 0.0076 N5 0.0204 0.0127 0.0086 O1 0.0953 0.0309 0.0121 O2 0.0135 0.0089 0.0080 P1 0.0111 0.0093 0.0075 P2 0.0135 0.0100 0.0075 P3 0.0373 0.0202 0.0083 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.065 0.100 0.130 0.156 0.182 0.212 0.248 0.292 0.380 1.000 Number in group 490. 493. 492. 483. 493. 480. 497. 477. 488. 490. GooF 1.189 1.287 1.116 1.148 0.997 1.039 0.877 0.812 0.822 0.734 K 1.020 1.019 0.995 1.003 0.992 1.010 1.006 1.016 1.005 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.63 inf Number in group 501. 481. 503. 472. 484. 499. 485. 480. 487. 491. GooF 1.054 1.021 1.104 0.991 0.889 0.827 0.872 0.724 0.953 1.521 K 0.995 1.014 1.012 1.012 1.017 1.015 1.012 1.001 1.008 1.001 R1 0.056 0.044 0.049 0.039 0.034 0.029 0.028 0.021 0.024 0.039 Recommended weighting scheme: WGHT 0.0460 1.0960 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -6 0 2 90.46 39.34 7.21 0.078 1.63 -1 0 5 104.22 54.73 6.02 0.092 2.31 -4 -3 2 220.38 129.37 5.95 0.142 1.97 -3 -1 5 100.93 55.14 5.51 0.093 2.10 -3 1 5 100.51 55.13 5.50 0.093 2.10 -4 3 2 216.16 135.72 5.18 0.145 1.97 0 2 1 139.06 222.13 4.62 0.186 4.56 4 1 1 97.79 61.33 4.34 0.098 2.08 0 0 4 75.04 46.32 4.14 0.085 2.74 0 -2 1 147.41 226.57 4.12 0.188 4.56 2 -3 0 219.87 320.49 4.06 0.223 2.71 2 0 2 453.74 329.54 3.91 0.226 3.07 -3 0 5 160.28 111.18 3.85 0.131 2.15 4 -1 1 97.57 64.58 3.81 0.100 2.08 0 12 1 38.48 66.86 3.79 0.102 0.83 -6 0 4 43.13 24.96 3.77 0.062 1.58 -9 5 11 86.81 51.53 3.71 0.089 0.80 -2 -2 3 203.15 286.16 3.67 0.211 2.86 0 0 5 437.22 594.13 3.57 0.304 2.19 2 3 0 219.86 308.41 3.54 0.219 2.71 -1 4 1 483.84 655.74 3.53 0.319 2.41 -2 4 2 947.74 721.14 3.50 0.335 2.17 -1 -4 1 478.64 648.31 3.48 0.317 2.41 6 -1 0 337.77 253.00 3.46 0.198 1.52 -1 -6 12 132.50 192.44 3.45 0.173 0.82 1 -4 5 13.68 5.06 3.44 0.028 1.56 -8 0 8 3.60 12.12 3.38 0.043 1.07 1 -12 0 287.17 212.48 3.36 0.182 0.83 5 0 0 42.36 26.17 3.35 0.064 1.85 1 12 5 56.91 31.63 3.32 0.070 0.77 -5 0 2 2554.37 2002.39 3.28 0.558 1.96 -4 -4 13 12.98 27.27 3.28 0.065 0.84 -2 -3 4 50.79 76.54 3.26 0.109 2.14 1 4 5 15.87 4.89 3.25 0.028 1.56 1 7 6 21.65 10.69 3.19 0.041 1.09 -8 -8 3 4.90 14.05 3.17 0.047 0.88 3 -8 5 14.34 29.88 3.16 0.068 0.98 1 -8 9 71.95 113.84 3.14 0.133 0.85 -2 3 4 54.08 79.73 3.12 0.111 2.14 -9 -6 9 21.37 10.38 3.12 0.040 0.83 1 8 9 77.09 117.36 3.11 0.135 0.85 3 0 7 6.87 1.81 3.10 0.017 1.24 2 12 4 27.86 45.92 3.10 0.084 0.78 -1 -4 4 199.89 151.03 3.09 0.153 1.90 3 5 0 286.46 220.18 3.02 0.185 1.68 -6 -10 8 68.73 46.09 3.02 0.085 0.78 -9 -4 11 55.01 85.80 3.01 0.115 0.82 -1 -9 7 46.96 71.85 3.00 0.106 0.92 6 1 0 331.06 255.84 3.00 0.199 1.52 -8 8 4 153.35 216.45 3.00 0.183 0.87 Bond lengths and angles C1 - Distance Angles N4 1.4755 (0.0030) C2 1.5288 (0.0035) 114.52 (0.21) C1 - N4 C2 - Distance Angles C3 1.5258 (0.0035) C1 1.5288 (0.0035) 117.18 (0.20) C2 - C3 C3 - Distance Angles O1 1.4570 (0.0027) C2 1.5258 (0.0035) 111.36 (0.19) C3 - O1 C4 - Distance Angles C5'_b 1.3455 (0.0075) N5 1.4406 (0.0036) 138.58 (0.43) C5_a 1.7006 (0.0064) 44.30 (0.34) 109.76 (0.32) C4 - C5'_b N5 C5_a - Distance Angles C6 1.4371 (0.0066) C4 1.7006 (0.0064) 110.49 (0.30) C5_a - C6 C5'_b - Distance Angles C4 1.3455 (0.0074) C6 1.5204 (0.0076) 128.48 (0.54) C5'_b - C4 C6 - Distance Angles O2 1.3469 (0.0049) C5_a 1.4371 (0.0066) 107.07 (0.36) C5'_b 1.5204 (0.0076) 134.91 (0.44) 47.54 (0.36) C6 - O2 C5_a C7 - Distance Angles C12 1.3939 (0.0036) C8 1.3970 (0.0037) 119.49 (0.22) P3 1.8030 (0.0022) 120.74 (0.18) 119.72 (0.20) C7 - C12 C8 C8 - Distance Angles C9 1.3891 (0.0038) C7 1.3970 (0.0037) 119.79 (0.30) C8 - C9 C9 - Distance Angles C10 1.3717 (0.0054) C8 1.3891 (0.0038) 121.03 (0.31) C9 - C10 C10 - Distance Angles C9 1.3717 (0.0054) C11 1.3836 (0.0051) 119.57 (0.24) C10 - C9 C11 - Distance Angles C10 1.3836 (0.0051) C12 1.3997 (0.0034) 120.62 (0.29) C11 - C10 C12 - Distance Angles C7 1.3939 (0.0036) C11 1.3997 (0.0034) 119.50 (0.26) C12 - C7 C13 - Distance Angles C18 1.3894 (0.0032) C14 1.3945 (0.0031) 119.46 (0.20) P3 1.8065 (0.0022) 119.68 (0.17) 120.63 (0.17) C13 - C18 C14 C14 - Distance Angles C15 1.3894 (0.0032) C13 1.3945 (0.0031) 120.41 (0.22) C14 - C15 C15 - Distance Angles C14 1.3894 (0.0032) C16 1.3905 (0.0038) 120.12 (0.24) C15 - C14 C16 - Distance Angles C17 1.3885 (0.0042) C15 1.3905 (0.0038) 119.77 (0.23) C16 - C17 C17 - Distance Angles C16 1.3885 (0.0042) C18 1.3992 (0.0035) 120.13 (0.25) C17 - C16 C18 - Distance Angles C13 1.3894 (0.0032) C17 1.3992 (0.0035) 120.11 (0.24) C18 - C13 N1 - Distance Angles P1 1.5984 (0.0019) P2 1.6044 (0.0019) 113.06 (0.10) N1 - P1 N2 - Distance Angles P2 1.5931 (0.0019) P3 1.6092 (0.0020) 121.36 (0.12) N2 - P2 N3 - Distance Angles P1 1.5800 (0.0019) P3 1.6204 (0.0019) 116.78 (0.12) N3 - P1 N4 - Distance Angles C1 1.4755 (0.0030) P1 1.6251 (0.0020) 122.71 (0.17) N4 - C1 N5 - Distance Angles C4 1.4406 (0.0036) P2 1.6311 (0.0020) 124.64 (0.20) N5 - C4 O1 - Distance Angles C3 1.4570 (0.0027) P2 1.5985 (0.0016) 119.13 (0.14) O1 - C3 O2 - Distance Angles C6 1.3469 (0.0049) O2 - P1 - Distance Angles N3 1.5800 (0.0019) N1 1.5984 (0.0019) 118.09 (0.10) N4 1.6251 (0.0020) 111.43 (0.11) 107.86 (0.11) Cl1 2.0357 (0.0008) 106.38 (0.08) 104.05 (0.07) 108.45 (0.09) P2 2.6718 (0.0007) 94.05 (0.07) 33.54 (0.07) 98.75 (0.08) 136.31 (0.03) P1 - N3 N1 N4 Cl1 P2 - Distance Angles N2 1.5931 (0.0019) O1 1.5985 (0.0016) 104.36 (0.09) N1 1.6044 (0.0019) 116.22 (0.10) 110.24 (0.09) N5 1.6311 (0.0020) 115.42 (0.11) 105.59 (0.10) 104.58 (0.11) P1 2.6718 (0.0007) 89.17 (0.07) 101.16 (0.06) 33.40 (0.06) 136.92 (0.08) P2 - N2 O1 N1 N5 P3 - Distance Angles N2 1.6092 (0.0020) N3 1.6204 (0.0019) 117.95 (0.10) C7 1.8030 (0.0022) 109.24 (0.11) 107.92 (0.11) C13 1.8065 (0.0022) 108.67 (0.11) 107.16 (0.10) 105.16 (0.10) P3 - N2 N3 C7 Cl1 - Distance Angles P1 2.0357 (0.0008) Cl1 - FMAP and GRID set by program FMAP 2 1 26 GRID -2.174 -2 -2 2.174 2 2 R1 = 0.0340 for 2585 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.22 at 0.4365 0.4452 0.4622 [ 0.83 A from C5 ] Deepest hole -0.52 at 0.3731 0.5707 0.4156 [ 0.55 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3145 / 24562 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5635 0.9452 0.5378 1.00000 0.05 1.22 0.83 C5 0.96 C6 1.05 H5B 1.36 H6A Q2 1 0.6844 0.9574 0.5344 1.00000 0.05 0.49 0.69 O2 0.72 H2 1.29 C6 1.71 C5 Q3 1 0.4057 0.9053 0.7093 1.00000 0.05 0.40 0.71 H4A 0.77 C4 1.02 H4B 1.69 C5' Q4 1 0.5528 1.1267 0.5571 1.00000 0.05 0.37 0.58 H6A 1.19 C6 1.48 H6B 2.02 O2 Q5 1 0.3023 0.6064 0.9356 1.00000 0.05 0.31 0.77 C3 0.79 C2 1.37 H2B 1.48 H3A Q6 1 0.4566 0.9568 0.4615 1.00000 0.05 0.30 1.17 H5B 1.50 H6A 1.62 C5 1.81 C6 Q7 1 0.7674 0.4538 0.7557 1.00000 0.05 0.29 0.74 C7 1.07 P3 1.87 C8 1.88 C12 Q8 1 0.6000 0.9141 0.7074 1.00000 0.05 0.26 0.50 C5' 0.55 H5'1 1.08 H5'2 1.36 C5 Q9 1 0.8073 0.3966 0.6827 1.00000 0.05 0.23 0.59 C7 0.83 C12 1.56 H12 1.72 C8 Q10 1 0.4108 0.5362 0.7034 1.00000 0.05 0.22 0.66 N1 1.11 P2 1.94 P1 2.11 N5 Q11 1 0.6089 0.3061 0.8099 1.00000 0.05 0.22 0.33 N3 1.73 P1 1.83 P3 2.61 H12 Q12 1 0.5310 1.1801 0.4912 1.00000 0.05 0.22 1.15 H6A 1.73 H5N 1.82 H5B 1.95 C6 Q13 1 0.4124 0.7459 0.9832 1.00000 0.05 0.21 1.36 H3B 1.43 H4N 1.44 O1 1.52 C3 Q14 1 0.4112 0.0867 0.7339 1.00000 0.05 0.20 1.57 CL1 1.73 H5'2 1.96 H4A 1.97 H4B Q15 1 0.6037 0.8966 0.4609 1.00000 0.05 0.20 1.19 H2 1.21 H5B 1.66 C5 1.74 O2 Q16 1 0.3944 0.4406 0.7152 1.00000 0.05 0.20 0.63 N1 1.07 P1 1.97 P2 2.18 H2 Q17 1 0.4622 0.8041 0.4748 1.00000 0.05 0.20 0.71 H5B 1.55 C5 2.03 H5A 2.20 H5N Q18 1 0.9784 0.3011 0.4283 1.00000 0.05 0.20 1.43 H10 1.86 H9 1.94 C10 1.99 H11 Q19 1 0.4705 1.1187 0.3848 1.00000 0.05 0.19 1.68 H6A 1.91 H5N 1.97 N2 2.02 P2 Q20 1 0.2780 0.4837 0.9469 1.00000 0.05 0.19 0.76 C1 0.77 C2 1.41 H1B 1.44 H2B Shortest distances between peaks (including symmetry equivalents) 4 12 0.90 10 16 0.99 1 6 1.13 2 15 1.13 7 9 1.19 1 15 1.19 1 2 1.20 5 20 1.27 12 17 1.30 12 19 1.33 6 17 1.54 6 15 1.56 15 17 1.72 5 13 1.74 1 17 1.74 4 17 1.81 3 14 1.84 1 4 1.84 6 19 1.88 4 19 1.89 1 8 1.91 3 8 1.91 10 19 1.97 4 6 2.08 15 16 2.10 2 6 2.11 2 4 2.20 10 15 2.33 6 12 2.35 7 11 2.37 1 12 2.42 17 19 2.42 11 16 2.43 1 19 2.44 2 8 2.45 11 13 2.55 2 17 2.57 15 19 2.59 8 14 2.62 6 9 2.64 2 12 2.65 4 15 2.68 12 15 2.69 4 8 2.70 16 19 2.70 2 10 2.72 6 7 2.74 2 16 2.75 6 10 2.76 2 19 2.76 6 8 2.77 1 12 2.80 8 17 2.81 9 17 2.82 6 12 2.83 4 14 2.86 11 14 2.87 8 15 2.88 7 19 2.88 6 16 2.88 10 12 2.89 13 20 2.91 1 3 2.92 9 11 2.94 12 15 2.98 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 2.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.99: Structure factors and derivatives 4.80: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.63: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0259 finished at 17:34:27 Total CPU time: 11.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++